Darstellung und Kristallstruktur von 2,4,6-Triferrocenyl- 1,3,5,2,4,6-triselenatriborinan/Synthesis and Crystal Structure of 2,4,6-Triferrocenyl-1,3,5,2,4,6-triselenatriborinane

1992 ◽  
Vol 47 (1) ◽  
pp. 1-4 ◽  
Author(s):  
Hans Horn ◽  
Frank Rudolph ◽  
Reinhart Ahlrichs ◽  
Kurt Merzweiler

The reaction of [(NEt3)FcBBr2] (Fc:C5H5FeC5H4) with bis(trim ethylsilyl)selenane leads to the formation of Fc3B3Se3 (1). 1 crystallizes in the triclinic space group P1̄. The lattice constants (at 210 K) are: a = 1487.8(8) pm , b = 1563.1(8) pm, c = 1588.6(9) pm, ɑ = 107.81(4)°, β = 101.06(4)°, γ = 115.85(4) . 1 contains a nearly planar B3Se3 ring with alternating B and Se atoms. The electronic structure of the model compound Ph3B3Se3 was investigated by ab initio SCF studies.

1990 ◽  
Vol 45 (4) ◽  
pp. 413-416 ◽  
Author(s):  
Johannes Beck

WCl6 reacts with two equivalents of tellurium in a sealed evacuated ampoule in the temperature range from 170 to 190 °C to give Te42+(WCl6-)2. Under the same conditions with one equivalent of tellurium WCl5 yields Te42+(WCl6-)2 and WCl4. Te4(WCl6), formes black crystals, which are sensitive to moist air. It decomposes at temperatures above 300° C to Te and WCl6. The crystal structure determination (lattice constants a = 638.9(1), b = 753.2(2), c = 1102.0(5) pm, α = 101.19(2)°, β = 102.85(2)°, γ = 90.21(1)°, Z = 1, triclinic space group P 1̄, 3572 unique reflections for 82 parameters, final R = 0.026) shows the nearly ideal square Te42+ cation with Te–Te distances of 268.8 and 268.7 pm and markedly distorted WCl6– octaedra with W–Cl bond length from 227.5 to 237.3 pm. The structure involves interionic Te–Cl contacts as short as 319 pm.


1993 ◽  
Vol 48 (12) ◽  
pp. 1732-1736 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher

The reaction of diisobutylamine, H2S, and sulfur in a mixture of dimethylformamide, formamide, and ethanol yields orange crystals of bis(diisobutylammonium)-heptasulfide. The compound crystallizes in the centrosymmetric orthorhombic space group Pbca, the lattice constants are a = 11.234(4), b = 17.875(7), c = 27.009(10) Å. The S72-chain does not have the common helical all-trans-conformation, but a mixed conformation trans-cis-trans (sequence of the signs of torsion angles + + - - and - - + +).


1985 ◽  
Vol 40 (6) ◽  
pp. 736-739 ◽  
Author(s):  
Herbert W. Roesky ◽  
Jörg Sundermeyer, ◽  
Jürgen Schimkowiak ◽  
Peter G. Jones ◽  
Mathias Noltemeyer ◽  
...  

AbstractThe reaction of N,N-dichlorophenylsulphonamide with tungsten hexacarbonyl in refluxing CCl4 leads in good yield to the yellow polymeric complex [(PhSO2N)2WCl2]x, which may be converted to the octahedral nitrene complex [(PhSO2N)2WCl2(CH3CN)2] by recrystallisation from aceto­nitrile. Crystals of the acetonitrile complex are triclinic, space group P 1̅, a = 820.7(2), b = 1128.8(3), c = 1286.9(3) pm, α = 89.25(3), β = 89.54(3). γ = 72.67(2)°, Z = 2, R = 0.027 for 2527 unique observed reflections.


1991 ◽  
Vol 46 (5) ◽  
pp. 699-702 ◽  
Author(s):  
Rolf Buschmann ◽  
Hans-Uwe Schuster

A new compound LiCo6P4 could be synthesized, it crystallizes in the hexagonal space group P6̅m2 with the lattice constants a = 658.4(3) pm, c = 333.8(2) pm, c/a = 0.507. The structure shows close relations to the Fe2P- or Zr2Fe12P7-type structures.


1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.


1995 ◽  
Vol 50 (8) ◽  
pp. 1175-1180 ◽  
Author(s):  
Hans-Christian Böttcher ◽  
Helmut Hartung ◽  
André Krug

[{Ru(CO)3Cl2}2] reacts with the in situ prepared reagent Li2[Fe(CO)3(PBut2)2] to give the new heterobinuclear complex [FeRu(CO)5(μ-PBut2)2] (1). Crystals of 1 are isomorphous to those of the known compound [Fe2(CO)5(μ-PBut2)2] (2) and crystallize in the triclinic space group P1̄ with a = 867,5(1), b = 1181,0(2), c = 1373,1(2) pm; α = 76,64(1), β = 79,72(1) and γ = 76,48(1)°. A double bond between the two metal atoms concluded for 2 from the results of EHMO calculations is also proposed for 1 (Fe=Ru: 259,8(1) pm).


1982 ◽  
Vol 37 (11) ◽  
pp. 1361-1368 ◽  
Author(s):  
H.-J. Schweizer ◽  
Reginald Gruehn

By using chemical transport reactions with various transporting agents (HgCl2, NbCl5, Nb3O7Cl) a slightly substoiehiometric NbO2-phase, β-NbO2, was obtained from samples with O/Nb ∼ 1.5 (source; T > 1373 K) and with deposition temperatures > 1273 K (sink). The rango of composition of β-NbO2 was found to exist from NbO1.990 to NbO1.998.The structure of the tetragonal, column-shaped black crystals was determined by X-ray diffraction. It crystallizes tetragonally in the space group I41 with lattice constants a = 9.693(3) Å, c = 5.985(1) Å and Z = 10 formula units.The crystal structure of β-NbO2 is shown to be a deformed rutile type. As in α-NbO2 the Nb-atoms are grouped in pairs. However, both oxides are different with respect to their long-range order.


1996 ◽  
Vol 51 (10) ◽  
pp. 1464-1468 ◽  
Author(s):  
Walter Frank ◽  
Guido J. Reiß

Tris(guanidinium) hexachlororhodate(III) monohydrate, [C(NH2)3]3[RhCl6] · H2O (1 ) has been obtained by the reaction of rhodium(III) chloride with guanidine hydrochloride in hydrochloric acid solution. 1 crystallizes in the triclinic space group P1̅ (a = 7.6013(9) Å, b = 8.6912(10) Å, c = 15.956(2) Å, α = 93.177(10)°, β = 101.691(10)°, γ = 113.995(9)°, V = 931.8(2), Z = 2). Two crystallographically independent hexachlororhodate ions, three crystallographically independent guanidinium ions and one water molecule are linked by a complex framework of hydrogen bonds.


1985 ◽  
Vol 40 (3) ◽  
pp. 443-446 ◽  
Author(s):  
Udo Demant ◽  
Elke Conradi ◽  
Ulrich Müller ◽  
Kurt Dehnicke

[HC(NH2)2]3FeCl6 was obtained together with other products from the reaction of S4N4 with HCl in H2CCl2 in the presence of FeCl3. Its crystal structure was determined from X-ray diffraction data (473 independent observed reflexions, R = 0.047). Lattice constants: a = 961.6, c = 876.4 pm; tetragonal, space group P42/m, Z = 2. Of the two crystallographically independent formamidinium ions HC(NH2)2⊕, one exhibits positional disorder; the other one has C-N bond lengths of 128 pm. The FeCl63⊖ ions have symmetry C2h, but the deviation from Oh is small.


1998 ◽  
Vol 63 (11) ◽  
pp. 1884-1892 ◽  
Author(s):  
Róbert Gyepes ◽  
Petr Štěpnička ◽  
Ulf Thewalt ◽  
Miroslav Polášek ◽  
Jiří Čejka ◽  
...  

Dimeric titanocene [(μ-η5:η5-C10H8){(μ-H)(η5-C5H5)Ti}2] (1) reacts with one equivalent of (trimethylsilyl)acetylene (TMSA) to give a mixture of diamagnetic (trimethylsilyl)acetylide-bridged compounds [(μ-η5:η5-C10H8)(μ-H)(μ-η1:η2-C≡CSiMe3){(η5-C5H5)Ti}2] (2) and [(μ-η5:η5-C10H8){(μ-η1:η2-C≡CSiMe3)(η5-C5H5)Ti}2] (3), and some oligomers of TMSA. Compound 2 crystallizes from hexane in the triclinic space group P1 (No. 2; a = 9.385(4) Å, b = 14.487(6) Å, c = 18.085(6) Å, α = 110.34(2)°, β = 101.56(2)°, γ = 96.65(3)°, V = 2 212(2) Å3, Z = 2). A highly soluble compound 3 could not be isolated from a mixture with oligomers of TMSA.


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